Textile process and product



Patented Jam- 19, 1937 berland, Md., assignorsto Celanese Corporationof America, a corporation of Delaware No Drawing. Application January 17, 1935,

' Serial No. 2,205

18 Claims.

This invention relates to the treatment of yarn and other textile materials and relates more particularly to the conditioning of yarns made of organic derivatives of cellulose whereby the same 5 may be successfully knitted into fabrics containing a large number of courses, or used in other textile operation lnwhich the yarn is susceptible to a great number of very sharp bends as in circular knitting. An object of the in o vention is to incorporate in yarns containing organic derivatives of cellulose a conditioning fluid whereby the same are rendered more pliable and, therefore, more suitable for use in textile operations where they are subjected to rather 15 sharp bends and turns. Other objects of the invention will appear from the following detailed description. I

The textile operations which require the yarn "to be flexed several times and through very 20 sharp angles as found in circular and warp knitting, present serious difficulties such as stitch distortion due to the lack of pliability of the yarn or the flufling of the yarn passing through the needles and guides of the machine. In order to condition such yarns animal, vegetable oil such as olive oil, or mineral oil have been applied thereto. Further, compounds containing animal, vegetable or mineral oils compounded with glycerides, fatty acids and other materials 30 have been applied to yarn. While these materials render such yarns pliable to a certain degree, after storage of the yarn for a period of time they develop either a gumminess on the yarn or a harshness in the yarn. Also yarns 35 lubricated with these materials in the customary manner and to the customary degree are difficult to circular knit into a fabric containing 45 or more courses per inch.

We have found that if there is incorporated 40 in the yarn a suflicient'quantity of conditioning fluid containing a softening agent for the organic derivative of cellulose and a lubricant, the yarns containing organic derivatives of cellulose may successfully be fabricated by circular knitting or otherwise into fabrics of very close stitch shape and that during such fabrication there is neither stitch distortion nor a breaking into holes due to the yarn breaking where theyare bent through a very sharp angle. Moreover,

9. degree may be stored for periods of a few weeks before fabricating them to a fabric without materially affecting the resulting product. 55 In accordance with our invention, we incorpoyarns treatedwith such a lubricant and to such rate in or apply as a coating to textile materials comprising filaments of cellulose acetate or other organic derivatives of cellulose at least 15%, based on the weight of the textile material, of a conditioning agent containing an ether of the 5 type hereinafter defined, which is a solvent or at least a latent solvent for the cellulose acetate or'other organic derivatives of cellulose, compounded with a lubricant material containing vegetable oils, animal oils and/or oxidized oils.

The textile materials to be made or treated. in accordance with our invention may be in the form of yarns containing a plurality of filaments made of cellulose acetate or other organic derivative of cellulose. These yarns may be composed of any number of individual filaments or the same may be composed of short lengths of filaments, for instance, staple fibers twisted together to form a yarn. Any degree of twist may be employed in the yarns. While we prefer to treat textile materials containing cellulose acetate, such textile materials may contain other organic derivatives of cellulose such as cellulose formate, cellulose propionate, cellulose butyrate, ethyl cellulose, methyl celluose and benzyl cellulose. If desired, the yarns or filaments thereof made or treated in accordance with this invention may have finely divided pigment like material such -.as titanium dioxide, antimony trioxide, stannic oxide, starch, high melting point insoluble organic compounds and the like incorporated therein in order to give them a subdued luster.

Yarns to be treated need not'consist wholly of filaments of cellulose acetate but may also con-' tain fibers of other materials such as natural silk, artificial fibers of reconstituted-cellulose. wool, cotton, etc. Yarns of cellulose acetate may be formed from continuous filaments or the same I may be spun from short staples or short lengths 40 I of such filaments.

The principal object of the present invention is to condition yarns comprising organic derivatives of cellulose, i. e. to treat such yarns with a suitable fluid so as to render them more pliable, sufficiently tacked together and suflicient- 1y lubricated and, therefore, more suited for use in textile operations requiring very fine stitch shapes or sharp bends of the material. It also results in an even tension on the yarnsas they pass through needles, guides, tensioning devices, etc. of the fabricating machines. In accordance with the invention, such conditioning is effected by treating the yarns with a compound which may be termed a lubricating compound. This 5 compound is preferably made of two or more ingredients, one of which has a softening action .or solvent action upon the organic derivative of cellulose and the other may or may not have these properties but has the property of lubrieating the yarn and wetting same. The solvent or softening agent to be incorporated in the lubricating compound is preferably. antype of ether. The type of ether referred to is an ether of the formula.

where R is hydrogen or an alkyl or phenyl residue and the two free oxygen bonds are linked to two monovalent radicals derived from polyhydric alcohols or from hydroxy-carboxylic acids or are linked to a divalent radical derived from a polyhydric alcohol or a hydroxy-carboxylic acid, and obtainable by the condensation of an aldehyde such as formaldehyde, acetaldehyde, butyraldehydeor benzaldehyde with an aliphatic hydroxy compound, for example, a polyhydric alcohol, a partial ether of a polyhydric alcohol, or an aliphatic hydroxy carboxylic acid. This type of ether is referred to hereinafter in the specification and in the claims as a formal-ether.

The formal-ether of the present invention may be made by the condensation of formaldehyde, formalin, tri-hydroxy-methylene, butraldehyde or paraformaldehyde in the presence or absence of an acid catalyst with simple polyhydric alcohols, such as glycerol, ethylene glycol or propylene glycol, or substituted polyhydric alcohols such as glyerolmono-chlorohydrine or di-ethylene glycol. Examples of partial ethers of polyhydric alcohols that may be employed for making the I formal-ether of the type above defined are the mono-methyl ether of ethylene glycol, the monoethyl ether of ethylene glycol, and the monomethyl or ethyl ether of propylene glycol or of diethylene glycol. Examples of hydroxy carboxylic acids that may be used for preparing the formal-ethers of the type above defined are alpha-hydroxy-iso-butyric acid, alpha-hydroxy normal butyric acid, glycollic acid, lactic acid, etc. Examples of acid catalysts that may be employed for promoting the condensation are ferric chloride or other acid salts, hydrochloric acid, sulphuric acid, phosphoric acid or. other strong or weak mineral acids.

Generally, it is preferable to employ these formal-ethers of the type hereinbefore defined that are relatively non-volatile, having a boiling point above, say, 140 C. and are soluble in or miscible with water. The reason that relatively non-volatile formal-ethers are preferred is'that upon the fabricating of the conditioned yarn such formal-ethers do not evaporate readily and, therefore, the treated'yarns retain their pliability for a long period of time. Since it is desirable that the formal-ethers which are solvents or latent solvents be removed from the fabric after" it is formed from the treated yarn if they are water soluble they can be readily removed in the ordinary scouring and/or dyeing operations and even exert a beneficial effect in such operations.

If desirable, the formal-ethers of the type hereinbefore defined may be employed in conjunction with other relatively high boiling solvents or latent solvents for organic derivatives of cellulose, suchv as ethyl oxybutyrate, benzyl alcohol. di-acetone alcohol, monacetin, diacetin,

acetyl carbinol, cyclopentanone, di-methyl tartrate, etc.

While one or more formal-ethers of the type herei-nbefore define-d may be incorporated in or applied to the textile materials alone, generally it is preferableto apply the same in admixture with one or more other conditoning agents, such as oil lubricants and relatively non-volatile materials having an aflinity for water. Since it is desirable that the organic derivative of cellulose yarn have thereon an oily lubricant to facilitate winding; twisting, knitting, weaving or other textile operations, it is preferred to incorporate in the conditioning or lubricating compounds along with the formal-ethers an oily material. The oily material may be any suitable oil or materials having the property of lubrication, it being preferred, however, to use a high percentage of an oil which does not readily oxidize or otherwise' change its properties to form large quantities of free acid on one hand or to polymerize and form gums on the other hand. Examples of suitable oils are olive oil, castor oil, teaseed oil, egg oil, soy bean oil, peanut oil, palm oil, cottonseed or other non-drying oils or other vegetable, animal or mineral oils. If the specific oils employed are not miscible with the specific formalether used they may generally be rendered miscible with each other and with any polyhydric alcohol and/or water present by the addition of a free fatty acid such as oleic acid or stearic acid,

or a cyclic hydrocarbon such as xylol.

The tendency of the oily material in the lubrieating compound to oxidize or otherwise change its properties is retarded by the presence of a formal-ether. It is of advantage, however, to employpre-oxidized vegetable oils, such as oxidized olive oil, oxidized castor oil, etc. The difiiculty of ageing of the ordinary oils is thus largely overcome and, moreover, such oxidized oils have greater miscibility with the formal-ether or a mixture of the formal-ether and a polyhydric alcohol in water than do normal oils. The oxidized oil may be prepared in any suitable manner, for instance, by injecting a fine stream of oxygen. into a body of olive oil or more preferably by injecting olive oil in a fine spray into a stream of oxygen until the required degree of oxidation has occurred.

As to the relative proportions of formal-ether to olive or other oil employed, these may vary within relatively wide limits depending upon the results desired, the proportions being generally from 50 to of formal-ether and 50 to 10% of olive oil ,or other oil.

To the yarn, as a, separate conditioning liquid or as a liquid mixed with the compounded lubricant, there may be applied a hygroscopic relatively non-volatile substance. This hygroscopic substance may be applied subsequently to the lubricant either with or without formal-ether. Ex-

amples of such hygroscopic substances are relayarn, this is very important when desiring to cir-v cular knit fabrics containing a large number of courses per inch. For example, in knitting the fabric that is to contain above 40 courses per inch in the finished fabric at least of the conditioning agent calculated as a mixture of formal-ether and vegetable oil is required. For best results in forming the fine stitch shapes from 15 to 25% or more of the conditioning liquid is required. Circular lmit fabrics may be made having as high as 56 to 60 courses per inch when employing yarns containing of the conditioning liquid consisting of formal-ether, oxidized olive oil and olive oil. It is found that the yarn must be wet to the point of saturation with the conditioning fluid for the best results.

The conditioning fluid may be applied to the yarn in any suitable manner. Thus it may be applied by the immersing of hanks of yarn to be treated in a bath containing the conditioning fluid. If desired, the conditioning fluid may be applied to the yarn while it is in transit from package to package. This may be done'by passing the yarn over pads or wicks that are impregnated with the conditioning fluid or by passing over rollers or discs, the bottoms of which are immersed in the conditioning fluid. The conditioning fluid may be dripped onto the yarns while they are in transit, and also the -yarns may be caused to dip into a bath containing the conditioning fluid while they areiii transit, prior to being wound onto a suitable package. Inanother form, the conditioning fluid may be applied as a spray onto cones, bobbins, pirns or other packages while the same are being wound, so that the spray is being continuously applied during the formation of the package. If desired, the

yarn may be treated at the spinning cabinet with the conditioning agent while it is being transmitted from the spinning cabinet in which it is spun from solutions of organic derivatives of cellulose and prior to being woundand/or wound and twisted into yarn.

The yarn treated in accordance with this invention is very pliable and flexible, and may be knitted, woven or subjected to any other suitable textile operations, to form knitted or woven fabric, hosiery, or other articles.

Cellulose acetate yarns treated in accordance with this invention have many important advantages. As stated, they are very pliable and flexible, and even after storage for a prolonged period of time, not only is this pliability or flexibility retained but in many instances is actually improved. Therefore irrespective of the age of the treated yarns, they can be readily rewound from their original package or subjected to any textile operation.

This yarn may be knitted on circular knitting machines or on warp knitting machines to produce fabrics of many wales and courses per unit length, which fabrics are substantially free of pin holes, distortions, tension lines, rowiness, etc., 1

and have a much better appearance than fabric made from untreated yarns. Cellulose acetate yarn when treated by. this invention may be knitted on certain circular knitting machines which are not capable of knitting untreated cellulose acetate yarn or cellulose acetate yarn finished by previous methods, to form a commercially satisfactory fabric and likewise may be netted successfully on lace-making machines to form highly satisfactory lace. Moreover, when yarn treated by this invention is exposed for several days to normal atmospheric conditions without any precautions whatever, the yarn still retains its good knitting properties. more, yarn treated by this invention may be knitted at a higher rate than yarn treated by previous methods. vThe .yarn may be processed regardless of humidity conditions and this renders the use of expensive humidifying apparatus unnecessary.

In order further to illustrate our invention and without being limited thereto, the following specific example is given:

Example Conditioning liquid is made as follows:--

Parts by weight The ether formed by the condensation of formaldehyde with the monomethyl ether of ethylene glycol 75 to 85 Oxidized olive oil 12 to 20 Olive oil 3 to 8 This conditioning liquid may be applied by means of wicks, rollers. discs or other suitable furnishing devices to the cellulose acetate filaments immediately after their leaving the dry spinning machine and prior to their being wound or twisted and wound, or it may be applied to the yarns during any subsequent textile operation. Yarn intended for fine knitting purposes may be conditioned with the above liquid by applying thereto 18 to 20% of the liquid based on the weight of the organic derivative of cellulose in the yarns. As this amount of lubricating compound forms a considerably thick coating, it is preferable to knit the yarn within days after the application of the lubricating compound thereto or to apply an additional lubricant just 4 before knitting.

Yarns of organic derivatives of cellulose may be formed containing therein from 3 to 10% of the conditioning liquid and then treated before knitting with from 10 to 20% as a coating to where R is hydrogen or an alkyl or phenyl residue, and where the two free oxygen bonds are linked to two monovalent radicals derived from Furtherpolyhydric alcohols or from hydroxy-carboxylic acids or are linked to a divalent radical derived from a polyhydric alcohol 'or a hydroXy-car- 7 having the formula linked to two monovalent radicals derived from polyhydric alcohols or fromhydroxy-carboxylic acids or are linked to a divalent radical derived from a polyhydric alcohol or a hydroxy-oarboxylic acid and an oil. v

3. Yarn containing an organic derivative of cellulose and -more than 15% on the weight of the organic derivative of cellulose of a lubricating compound comprising an ether having the formula where R is hydrogen or an alkyl or phenyl residue, and where the two free oxygen bonds are linked to two monovalent vradicals'derived from polyhydric alcohols or from hydroxy-carboxylic acids or are linked to a divalent radical derived from a polyhydric alcohol or a hydroxy-car boxylic acid and an oxidized oil. 1

4. Yarn containing cellulose acetate and more than 15% on the weight of the cellulose acetate of a lubricating compound Icomprising an ether having the formula F where R is hydrogen or an alkylor phenyl residue, and where the two free'oxygen bonds are linked to two monovalent radicals derived from polyhydric alcohols or from hydroxy-carboxylic acids or are linked to a'divalent radical derived from a polyhydric alcohol or a-hydroxy-carboxylic acid and an oxidizedoil.

5. Yarn containing an organic derivative of cellulose and more than 15% on the weight of the organic derivative of cellulose of a lubricating compound comprising at least 50% of an ether having the formula where R is hydrogen or an alkyl or phenyl residue, andwhere the two free oxygen bonds are linked to two monovalent radicals derived from polyhydric alcohols or from hydroxy-carboxylic acids or are linked to a divalent radical derived from a polyhydric alcohol or a hydroxy-carboxylic acid and an oil.

6.. Yarn containing cellulose acetate and more than 15% on the weight of the cellulose acetate of a lubricating compound comprising at least compound containing; ether having the mp mula 50% of an ether having the formula where R is hydrogen or an alkyl or phenyl residue, and where the two free oxygen bonds are linked to two monovalent radicals derived from polyhydric alcohols or from hydroxy-carboxylic' acids or are linked to a divalent radical derived from a polyhydric alcohol or a hydroxy-carboxylic acid and an oil.

7. Yarn containing an organic derivative of cellulose and more than 15% on the weight of the organic derivative of cellulose of a lubricating compound comprising the condensation product of formaldehyde with the mono-methyl ether of ethylene glycol, and an oil.

8. Yarn containing cellulose acetate and more than 15% on the weight of the cellulose acetate of a lubricating compound comprising the condensation product of formaldehyde with. the mono-methyl ether of ethylene glycol, and an oil.

9. Yarn containing an organic derivative of cellulose and from 18 to '20% on the weight of the organic derivative of cellulose of a lubricating compound comprising an ether having the formula L t where R is hydrogen or an alkyl or phenyl residue, and where the two free oxygen bonds are linked to two monovalent radicals derived from polyhydric alcohols or from hydroxy-carboxylic acids or are linked to a divalent radical derived where R is hydrogen or an alkyl or phenyl residue, and where the two free oxygen bonds are linked-to two monovalent radicals derived from polyhydric alcohols or from hydroxy-carboxylic acids or. are linked to a divalent radical derived from a polyhydric alcohol or a hydroxy-carboxylic acid and an oil.

11. A fabric formed from yarns containing organic derivatives of cellulose and at least 15% of a lubricating compound containing an ether having the formula I where R is hydrogen'or an alkyl or phenyl residue, and where the two free oxygen bonds are linked to two monovalent radicals derived from polyhydric alcohols onfrom hydroxy-carboxylic acids orare linked to a divalent radical derived from a polyhydric alcohol or a hydroxy-carboxylic acid-and an oil.

1 2. A fabric formed from yarns containing'cellulose acetate and at least 15% of a lubricating where R is hydrogen or an alkyl or phenyl residue, and where the two free oxygen bonds are linked to two monovalent radicals derived from polyhydric alcohols or from hydroxy-carboxylic acids or are linked to a divalent radical derived from a polyhydric alcohol or a hydroxy-carboxylic acid and an oil.

13. Yarn containing organic derivative of cellulose filaments containing a metallic salt, said ,yarn having a coating of at least 15% its weight of a lubricating compound containing an ether having the formula where R is hydrogen or an alkyl or phenyl residue, and where the two free oxygen bonds are linked to two monovalent radicals derived from polyhydric alcohols or from hydroxy-carboxylic acids or are linked to a divalent radical derived from a polyhydric alcohol or a hydroxy-carboxylic acid and an oil.

15. Yarn containing an organic derivative .of cellulose and more than 15%, based on the weight of the derivative of cellulose present, of a lubrieating compound comprising an oil, an oxidized oil and an ether having the formula where R is hydrogen or an alkyl or phenyl residue, and where the two free oxygen bonds are linked to two monovalent radicals derived from polyhydric alcohols or from hydroxy-carboxylic acids-or are linked to a divalent radical derived from a polyhydric alcohol or a hydroxy-carboxylic acid.

16. Yarn containing cellulose acetate and more than 15%, based on the weight of the cellulose acetate present, of a lubricating compound comprising an oil, an oxidized oil and an ether having the formula where R is hydrogen or an alkyl or phenyl residue, and where the two free oxygen bonds are linked to two monovalent radicals derived from polyhydric alcohols or from hydroxy-carboxylic acids or are linked to a divalent radical derived from a polyhydric alcohol or a hydroxy-car- 'boxylic acid.

I 17. Yarn containing an organic derivative of cellulose and more than 15%, based on the weight of the organic derivative of cellulose present, of a lubricating compound comprising the condensation product of formaldehyde with the monomethyl ether of ethylene glycol, olive oil and oxid'ized olive oil.

18. Yarn containing cellulose acetate and more than 15%, based on the weight of the cellulose acetate present, of a lubricating compound comprising the condensation product offormaldehyde with the mono-methyl ether of ethylene glycol, olive oil and oxidized olive oil.

GEORGE R. BLAKE. GEORGE W. SEYMOUR. 

